US8293386B2 - Al-Ti-Ru-N-C hard material coating - Google Patents

Al-Ti-Ru-N-C hard material coating Download PDF

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Publication number
US8293386B2
US8293386B2 US12/667,171 US66717108A US8293386B2 US 8293386 B2 US8293386 B2 US 8293386B2 US 66717108 A US66717108 A US 66717108A US 8293386 B2 US8293386 B2 US 8293386B2
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Prior art keywords
hard material
material coating
coating according
coating
ruthenium
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Expired - Fee Related, expires
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US12/667,171
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English (en)
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US20100190032A1 (en
Inventor
Martin Kathrein
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Ceratizit Austria GmbH
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Ceratizit Austria GmbH
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Assigned to CERATIZIT AUSTRIA GESELLSCHAFT M.B.H. reassignment CERATIZIT AUSTRIA GESELLSCHAFT M.B.H. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KATHREIN, MARTIN
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/16—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
    • Y10T428/2495—Thickness [relative or absolute]
    • Y10T428/24967—Absolute thicknesses specified
    • Y10T428/24975—No layer or component greater than 5 mils thick
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less

Definitions

  • the invention relates to a single-layer or multilayer nitridic or carbonitridic hard material coating containing Al and Ti.
  • Highly wear-resistant hard material layers are applied to bodies subject to wear, in particular wear parts and tools, to increase the wear resistance. These coatings usually have hardness values in the range from 15 to above 40 GPa.
  • Hard materials which have been found to be useful include carbides, carbonitrides, nitrides and oxides, which are often employed together as mutually supplementary layers in a layer arrangement.
  • layers of different hard materials are arranged alternately in order to meet various requirements in respect of adhesion, wear and toughness.
  • Substrate bodies used are wear-resistant materials such as cemented carbides, cermet materials, hard materials and tool steels.
  • (Al x Ti 1-x )(N y C 1-y ) coatings which combine excellent wear properties with high oxidation resistance have been found to be useful.
  • the addition of Al to TiN increases the coating hardness and improves the oxidation resistance. At x>0.75, the coating hardness decreases due to the formation of hexagonal phase. At x ⁇ 0.56, the oxidation start temperature drops to below 800° C.
  • (Al x Ti 1-x )(N y C 1-y ) coatings can be produced by means of physical (PVD) or chemical vapour deposition (thermal CVD, PACVD).
  • PVD physical
  • PACVD chemical vapour deposition
  • a preferred PVD process is magnetron sputtering.
  • metallic Al—Ti targets which can be in alloyed form or in the form of composite target, are atomized using reactive gases and (Al x Ti 1-x )(N y C 1-y ) is deposited in this way.
  • the (Al x Ti 1-x )(N y C 1-y ) phases formed are generally metastable and form coherent precipitates in the temperature range from 600° C. to 1000° C., as a result of which self-hardening can be achieved during use at high temperatures.
  • the composition of the deposited coating is determined predominantly by the composition of the sputtering target.
  • the coating can contain further constituents, for example proportions of a process gas,
  • the hard material coating can have a single-layer or multilayer structure.
  • At least one coating layer has the composition (Al x Ti y Ru z Me v ) (N a C 1-a ), where
  • Me is at least one element from the group consisting of Si, B, W, Mo, Cr, Ta, Nb, V, Hf and Zr. If a plurality of elements are selected from this group, v is the total content of these elements.
  • the metals titanium and/or aluminum in the AlTiN or AlTiNC matrix are replaced by ruthenium.
  • ruthenium content is too low (z ⁇ 0.001), a satisfactory effect can no longer be determined.
  • ruthenium contents z>0.1
  • the room temperature hardness drops as a result of formation of hexagonal phase.
  • high ruthenium contents are not economically sensible because of the high price of ruthenium.
  • the preferred content of ruthenium is 0.005 ⁇ z ⁇ 0.06.
  • the hard material coating can be made up of one or more layers having a different composition and/or structure. At least one coating layer has the composition according to the invention.
  • the optimal silicon and boron content is, based on the proportion of metal, from 0.1 to 1 atom %, the optimal chromium, tungsten and molybdenum content is from 1 to 10 atom % and the optimal vanadium, niobium, tantalum, zirconium and hafnium content is from 1 to 20 atom %.
  • the addition of these elements increases the coating hardness in a concentration range where the cubic phase is predominantly present and generally reduces the coating ductility.
  • the composition therefore has to be matched to the application, with recourse being able to be made to experience with ruthenium-free coatings.
  • the ruthenium-containing coating or layer does not contain any further metallic elements apart from aluminum and titanium.
  • the inventive advantage of the addition of ruthenium is observed both in the case of nitrides and in the case of carbonitrides.
  • the cubic lattice is the dominant crystal structure.
  • dominant means that the proportion of cubic phase is greater than 50%.
  • small proportions of X-ray-amorphous and hexagonal phases can occur in addition to the cubic phase without the advantages of the invention being significantly reduced.
  • a ruthenium-containing layer preferably alternates with a ruthenium-free layer.
  • the ruthenium-containing layer has a ruthenium content of 0.005 ⁇ z ⁇ 0.05.
  • the aluminum content is 0.62 ⁇ x ⁇ 0.72 and the titanium content is 0.27 ⁇ y ⁇ 0.39.
  • the ruthenium-free layer has an aluminum and titanium content of 0.45 ⁇ x,y ⁇ 0.55.
  • the ruthenium-free intermediate layer is once again preferably cubic, with the cubic phase being able to be achieved by means of an Al:Ti ratio of from 0.8 to 2 and/or by adjusting the process parameters.
  • the bias voltage should once again be emphasized and preferably has a value of ⁇ 40 volt.
  • the cubic ruthenium-free intermediate layer makes it possible to increase the aluminum content in the ruthenium-containing layer without the proportion of hexagonal phase becoming unacceptably high.
  • the coating of the invention is, in preferred embodiments, deposited on cubic boron nitride or cemented carbide. It is possible to use the customary bonding layers, for example TiN, and covering layers, for example aluminum oxide or aluminum mixed oxides.
  • the preferred coating thickness is from 3 to 14 ⁇ m and the ruthenium content is 0.01 ⁇ z ⁇ 0.06. In the case of milling tools, the preferred coating thickness is from 2 to 8 ⁇ m and the ruthenium content is 0.005 ⁇ z ⁇ 0.02.
  • PVD processes As preferred deposition processes, mention may be made of PVD processes and among these plasma-supported gas-phase coating deposition processes, for example magnetron sputtering, electron evaporation, ion plating or laser-supported PVD processes. Arc vaporization processes are also suitable, especially in the development phase for determining optimal coating compositions.
  • the metallic elements deposited in the coating have a composition which is generally very close to the composition of the material used for the target.
  • composition of the coating according to the invention will consequently be defined by the composition of the target.
  • FIG. 1 shows the operating life of cemented carbide specimens in a longitudinal turning experiment.
  • the end of the operating life is specified as a wear width on the main cutting edge of 0.2 mm.
  • FIG. 2 a shows the wear after longitudinal turning experiments (hot-working steel W300) using an uncoated c-BN specimen (prior art) after a use time of 13 min.
  • FIG. 2 b shows the wear after longitudinal turning experiments (hot-working steel W300) using a c-BN specimen coated according to the invention after a use time of 13 min.
  • FIG. 2 c shows the wear after longitudinal turning experiments (hot-working steel W300) using a c-BN specimen coated according to the invention after a use time of 19 min.
  • FIG. 3 shows the wear width versus use time for longitudinal turning experiments (gray cast iron GG25) using uncoated c-BN specimens and c-BN specimens coated according to the invention.
  • FIG. 4 shows the operating life of cemented carbide milling tools.
  • the end of the operating life is specified as a wear width on the main cutting edge of 0.3 mm.
  • Cemented carbide tips having the composition WC, 9.6% by weight of Co, 7.3% by weight of mixed carbides of the type CNMG 120408 EN-TM were produced and provided by means of arc vaporization with coatings having the following composition:
  • the samples were produced in a production-scale Oerlikon Balzers RCS PVD unit.
  • the ruthenium-containing sputtering targets used were produced by powder metallurgy.
  • the multilayer coatings according to the invention were produced by replacing a target by a target having a composition according to the invention with otherwise identical process parameters.
  • the specimens used were in each case positioned in the same positions in the coating reactor.
  • the specimens 4 and 5 according to the invention have a superior wear resistance.
  • Cemented carbide indexable inserts of the type DCMW 11T304 with tips of cubic boron nitride were provided with a coating according to the invention as per specimen 4 in Example 1 and compared with uncoated tips.
  • the hot-working steel W 300 (DIN 1.2343) was machined dry.
  • the cutting speed v c was 200 m/min
  • the feed f was 0.05 mm
  • the advance depth was 0.3 mm.
  • gray cast iron of the grade GG 25 (DIN 0.6025) was likewise machined dry.
  • the cutting speed v c was 350 m/min
  • the feed f was 0.2 mm
  • the advance depth was 1.0 mm.
  • FIG. 2 the specimen according to the invention ( FIG. 2 b, c ) shows a significantly more favourable cratering behaviour. A significant increase in operating life compared to the uncoated hard material c-BN ( FIG. 2 a ) is therefore achieved.
  • FIG. 3 shows, both the wear on the flank of the main cutting edge (MCEW) and the wear on the face, referred to as crater wear, are reduced.
  • MCEW main cutting edge
  • FIG. 3 thus shows that the ruthenium-containing coating according to the invention deposited on a cubic boron nitride substrate material results in a significant increase in the operating life compared to an uncoated specimen.
  • Cemented carbide tips having the composition WC, 9.0% by weight of Co, 4.0% by weight of mixed carbides of the type SEKN 1203AFSN were provided with a coating according to the invention as per specimen 4 in Example 1 and a coating according to the prior art (specimen 3 in Example 1) and subjected to a comparable cutting machining test.
  • a 42CrMo4 steel (1.7225) having a strength of 1100 MPa was milled dry by means of a milling tool having a diameter of 160 mm using a cutting speed v c of 230 m/min, a feed per tooth f t of 0.3 mm and an advance a p of 2 mm in the single-tooth climb milling mode.
  • the termination criterion for the cutting machining experiments was set at a wear width of 0.3 mm on the flank of the main cutting edge.
  • FIG. 4 shows, a significant improvement in the operating life of the specimen coated according to the invention compared to the specimen according to the prior art was also able to be achieved here.
  • the composition of the ruthenium-containing coating is shown in Table 1. The thickness of the individual layers was 7 nm, and the total coating thickness was 5.2 ⁇ 0.8 ⁇ m. The coated samples were subjected to a comparative cutting machining test as per Example 3.
  • the operating life values in Table 1 show that an improvement in the coating properties can be achieved in the application by addition of further metallic alloying components.
  • further alloying components can be associated with a decrease in the ductility values and the influence of the ductility properties on the operating life behaviour is very specific to the application, the selection of the alloying element and the content thereof is dependent on the respective application.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Vapour Deposition (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
US12/667,171 2007-06-29 2008-06-26 Al-Ti-Ru-N-C hard material coating Expired - Fee Related US8293386B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
ATGM408/2007 2007-06-29
AT0040807U AT9999U1 (de) 2007-06-29 2007-06-29 Al-ti-ru-n-c hartstoffschicht
PCT/AT2008/000231 WO2009003206A2 (de) 2007-06-29 2008-06-26 Al-Ti-Ru-N-C HARTSTOFFSCHICHT

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US20100190032A1 US20100190032A1 (en) 2010-07-29
US8293386B2 true US8293386B2 (en) 2012-10-23

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US (1) US8293386B2 (de)
EP (1) EP2179073B1 (de)
JP (1) JP5450400B2 (de)
CN (1) CN101688299B (de)
AT (2) AT9999U1 (de)
DE (1) DE502008001850D1 (de)
ES (1) ES2351543T3 (de)
IL (1) IL203000A (de)
PL (1) PL2179073T3 (de)
WO (1) WO2009003206A2 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9321117B2 (en) 2014-03-18 2016-04-26 Vermeer Manufacturing Company Automatic system for abrasive hardfacing

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102012107129A1 (de) * 2012-08-03 2014-02-06 Walter Ag TiAIN-beschichtetes Werkzeug
US9476114B2 (en) 2012-08-03 2016-10-25 Walter Ag TiAlN-coated tool
DE102012017731A1 (de) 2012-09-08 2014-03-13 Oerlikon Trading Ag, Trübbach Ti-Al-Ta-basierte Beschichtung mit einer verbesserten Temperaturbeständigkeit
JP6102653B2 (ja) * 2013-09-19 2017-03-29 三菱マテリアル株式会社 表面被覆切削工具
EP3631040B1 (de) 2017-05-23 2023-10-25 Oerlikon Surface Solutions AG, Pfäffikon Dicke tialtan/alcrn-mehrschichtlackierungen auf turbinenbauteilen
CN116288191A (zh) * 2023-03-14 2023-06-23 纳狮新材料有限公司杭州分公司 一种高温抗氧化AlTiN基纳米涂层及其制备方法

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US4680438A (en) * 1985-03-14 1987-07-14 W. C. Heraeus Gmbh Laminated material for electrical contacts and method of manufacturing same
JPH0331471A (ja) * 1989-06-28 1991-02-12 Daido Steel Co Ltd 金色外装部品及びその製法
JPH08199340A (ja) 1995-01-20 1996-08-06 Hitachi Tool Eng Ltd 被覆硬質合金
JPH08199341A (ja) 1995-01-20 1996-08-06 Hitachi Tool Eng Ltd 被覆硬質合金
JPH08209332A (ja) 1988-03-24 1996-08-13 Kobe Steel Ltd 耐摩耗性に優れた工具を製造する方法
RU2070610C1 (ru) * 1993-05-07 1996-12-20 Научно-производственное государственное предприятие "Синтез" при Донском государственном техническом университете Многослойный материал для покрытия
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US20040076856A1 (en) 2000-11-16 2004-04-22 Hakan Hugosson Surface coating of a carbide or a nitride
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US4680438A (en) * 1985-03-14 1987-07-14 W. C. Heraeus Gmbh Laminated material for electrical contacts and method of manufacturing same
JPH08209332A (ja) 1988-03-24 1996-08-13 Kobe Steel Ltd 耐摩耗性に優れた工具を製造する方法
JPH0331471A (ja) * 1989-06-28 1991-02-12 Daido Steel Co Ltd 金色外装部品及びその製法
RU2070610C1 (ru) * 1993-05-07 1996-12-20 Научно-производственное государственное предприятие "Синтез" при Донском государственном техническом университете Многослойный материал для покрытия
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JPH08199340A (ja) 1995-01-20 1996-08-06 Hitachi Tool Eng Ltd 被覆硬質合金
JPH08199341A (ja) 1995-01-20 1996-08-06 Hitachi Tool Eng Ltd 被覆硬質合金
US6250855B1 (en) * 1999-03-26 2001-06-26 Sandvik Ab Coated milling insert
US20040076856A1 (en) 2000-11-16 2004-04-22 Hakan Hugosson Surface coating of a carbide or a nitride
US6824601B2 (en) * 2000-12-28 2004-11-30 Kobe Steel, Ltd. Hard film for cutting tools, cutting tool coated with hard film, process for forming hard film, and target used to form hard film
DE10109634C1 (de) 2001-03-01 2002-10-10 Boart Hwf Gmbh Co Kg Hartmetallkörper mit Wolframcarbid in Form von Platelets für Erd- oder Bodenbearbeitungswerkzeuge
US7056602B2 (en) * 2002-09-04 2006-06-06 Seco Tools Ab Precipitation hardened wear resistant coating
WO2006023222A1 (en) 2004-08-20 2006-03-02 Tdy Industries, Inc. Pvd coated ruthenium featured cutting tools
US7244519B2 (en) 2004-08-20 2007-07-17 Tdy Industries, Inc. PVD coated ruthenium featured cutting tools
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9321117B2 (en) 2014-03-18 2016-04-26 Vermeer Manufacturing Company Automatic system for abrasive hardfacing

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DE502008001850D1 (de) 2010-12-30
IL203000A (en) 2014-07-31
PL2179073T3 (pl) 2011-04-29
CN101688299A (zh) 2010-03-31
WO2009003206A3 (de) 2009-02-19
EP2179073B1 (de) 2010-11-17
ATE488617T1 (de) 2010-12-15
ES2351543T3 (es) 2011-02-07
EP2179073A2 (de) 2010-04-28
CN101688299B (zh) 2012-02-08
JP2010531928A (ja) 2010-09-30
AT9999U1 (de) 2008-07-15
US20100190032A1 (en) 2010-07-29
WO2009003206A2 (de) 2009-01-08
JP5450400B2 (ja) 2014-03-26

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